反应详情

5955 g 2-nitrobenzaldehyde was suspended in 10 L methanol under nitrogen atmosphere and 7500 g 4-amino-1-benzyl-piperadine in 5 L methanol was added over 30 min. The reaction was stirred 1 h at RT. The reaction mixture was cooled to 0° C. and a cold solution of 1044 g sodium borohydride in 6425 mL water was added at a rate to keep the temperature below 10° C. After 1 h stirring at 0° C. and 1 h at RT the reaction was cooled again to 0° C. and aqueous 4 mol/L hydrochlorid acid was added. Then the reaction mixture was stirred at RT for 30 min and cooled again to 0-10° C. Aqueous 5 mol/L sodium hydroxide solution was added until pH=14 and the reaction was extracted with tert-butyl methylether. The organic layer was washed with water and saturated sodium chloride solution and the solvent was evaporated. The residue was dissolved in toluol, filtered and concentrated again to yield 12.8 kg of the desired product.

1. temperatureThe reaction mixture was cooled to 0° C.
2. customthe temperature below 10° C
3. stirringAfter 1 h stirring at 0° C. and 1 h at RT the reaction
4. temperaturewas cooled again to 0° C.
5. stirringThen the reaction mixture was stirred at RT for 30 min
6. temperaturecooled again to 0-10° C
7. extractionthe reaction was extracted with tert-butyl methylether
8. washThe organic layer was washed with water and saturated sodium chloride solution
9. customthe solvent was evaporated
10. dissolutionThe residue was dissolved in toluol
11. filtrationfiltered
12. concentrationconcentrated again